硫脲介质-火焰原子吸收光谱法连续测定多金属矿石中的银镉
|
摘要
传统火焰原子吸收光谱法测定Ag、Cd,样品需单独处理,耗时且成本高。建立了火焰原子吸收光谱法连续测定多金属矿石中银、镉的方法,样品经盐酸、硝酸(氟化氢铵)分解,盐酸提取可溶性盐,在硫脲介质中火焰原子吸收光谱仪连续测定Ag、Cd。方法检出限分别为Ag 0.005 4μg/m L、Cd 0.003 2μg/m L,Ag、Cd测定结果的相对标准偏差分别为0.7%~2.8%、0.4%~2.4%,加入标准物质回收率分别为97.5%~103.6%、96.4%~104.0%。该方法酸的用量少,环境污染程度低,准确度和精密度良好。
Conventional FAAS takes much time and cost to determine Ag and Cd in ores because the samples need to be processed alone. In light of that,a continuous determination of Ag and Cd in polymetallic ores by FAAS is developed. The samples are dissolved by hydrochloric acid,nitric acid( ammonium bifluoride) and dissolvable salts are extracted with hydrochloric acid. And then,Ag and Cd are continuously determined by FAAS in thiourea media. The detection limits of the method are 0. 005 4 μg/mL for Ag and 0. 003 2 μg/mL for Cd. The RSD is 0. 7 %-2. 8 % for Ag and 0. 4 %-2. 4 % for Cd. The recovery rate of reference material is 97. 5 %-103. 6 % and 96. 4 %-104. 0 %respectively. The method consumes less acids,contains environment pollution and has good accuracy and precision.
Conventional FAAS takes much time and cost to determine Ag and Cd in ores because the samples need to be processed alone. In light of that,a continuous determination of Ag and Cd in polymetallic ores by FAAS is developed. The samples are dissolved by hydrochloric acid,nitric acid( ammonium bifluoride) and dissolvable salts are extracted with hydrochloric acid. And then,Ag and Cd are continuously determined by FAAS in thiourea media. The detection limits of the method are 0. 005 4 μg/mL for Ag and 0. 003 2 μg/mL for Cd. The RSD is 0. 7 %-2. 8 % for Ag and 0. 4 %-2. 4 % for Cd. The recovery rate of reference material is 97. 5 %-103. 6 % and 96. 4 %-104. 0 %respectively. The method consumes less acids,contains environment pollution and has good accuracy and precision.
引文
[1]薛光,任文生,薛元昕.金银湿法冶金及分析测试方法[M].北京:科学出版社,2009.
[2]《岩石矿物分析》编写组.岩石矿物分析:第一分册[M].北京:地质出版社,1991.
[3]代素芳,郑浩.在高氯酸-酒石酸-硫脲介质中原子吸收法测定多种矿石中的银[J].岩矿测试,2000,19(4):301-303.
[4]余煜棉,张俊浩,莫胜钧.溶剂萃取石墨炉原子吸收光谱法连续测定地质样品中金、银、镓、铟[J].光谱学与光谱分析,1996,16(3):99-104.
[5]张彦斌,程忠洲,李华.硫脲树脂富集-电感耦合等离子体质谱法测定地质样品中的超痕量金、银、铂、钯[J].分析试验室,2006,25(7):105-108.
[6]常平,王松君,孙春华,等.电感耦合等离子体原子发射光谱法测定黄铁矿石中微量元素[J].岩矿测试,2002,21(4):304-306.
[7]付冉冉,刘水清,荣德福,等.原子荧光光谱法测定铁矿石中的镉[J].岩矿测试,2009,28(6):595-597.
[8]折书群,谢俊霞.碘化钾-乙醇萃取火焰原子吸收法测定痕量银和镉[J].黄金,2003,24(3):51-52.
[9]黄俭惠,卢汉堤.火焰原子吸收光谱法测定高锑烟尘中的银、铅、镉[J].中国无机分析化学,2014,4(4):28-31.
[10]李占江.金银及有色金属地勘矿冶分析手册[M].北京:地质出版社,2013.
[11]邱宏喜,付桂花,谢璐,等.绿色化学法在金矿地质样品分析中的应用研究[J].黄金科学技术,2015,23(3):78-82.
[2]《岩石矿物分析》编写组.岩石矿物分析:第一分册[M].北京:地质出版社,1991.
[3]代素芳,郑浩.在高氯酸-酒石酸-硫脲介质中原子吸收法测定多种矿石中的银[J].岩矿测试,2000,19(4):301-303.
[4]余煜棉,张俊浩,莫胜钧.溶剂萃取石墨炉原子吸收光谱法连续测定地质样品中金、银、镓、铟[J].光谱学与光谱分析,1996,16(3):99-104.
[5]张彦斌,程忠洲,李华.硫脲树脂富集-电感耦合等离子体质谱法测定地质样品中的超痕量金、银、铂、钯[J].分析试验室,2006,25(7):105-108.
[6]常平,王松君,孙春华,等.电感耦合等离子体原子发射光谱法测定黄铁矿石中微量元素[J].岩矿测试,2002,21(4):304-306.
[7]付冉冉,刘水清,荣德福,等.原子荧光光谱法测定铁矿石中的镉[J].岩矿测试,2009,28(6):595-597.
[8]折书群,谢俊霞.碘化钾-乙醇萃取火焰原子吸收法测定痕量银和镉[J].黄金,2003,24(3):51-52.
[9]黄俭惠,卢汉堤.火焰原子吸收光谱法测定高锑烟尘中的银、铅、镉[J].中国无机分析化学,2014,4(4):28-31.
[10]李占江.金银及有色金属地勘矿冶分析手册[M].北京:地质出版社,2013.
[11]邱宏喜,付桂花,谢璐,等.绿色化学法在金矿地质样品分析中的应用研究[J].黄金科学技术,2015,23(3):78-82.